气相色谱-质谱法测定塑料制品中1,2-苯二酸-二烷基酯类的含量  

GC-MS Determination of 1,2-Benzene Dicarboxylic Acid-Dialkyl Esters in Plastic Products

作　　者：王桂苓 梁永明 刘贝贝 WANG Guiling;LIANG Yongming;LIU Beibei(National Quality Supervision and Inspection Center for Recycle Nonferrous Metals Rubber ~ Plastic Materials, Fuyang 236000, Chin)

机构地区：[1]国家再生有色金属橡塑材料质量监督检验中心(安徽),阜阳236000

出　　处：《理化检验（化学分册）》2018年第4期449-454,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：2014年度安徽省地方标准制修订项目;2015年阜阳市科技计划项目

摘　　要：建立了测定塑料制品中1,2-苯二酸-二(C6-8支链)烷基酯(富C7)(DIHP)和1,2-苯二酸-二(C7^(-1)1支链与直链)烷基(醇)酯(DHNUP)含量的气相色谱-质谱法。以乙酸乙酯20mL为提取剂提取样品(0.500 0g),于100℃微波萃取30 min,取提取液2.0 mL用乙酸乙酯定容至5.0mL,过滤后,在选择离子监测(SIM)模式下扫描,用气相色谱-质谱法进行测定,以特征碎片离子的丰度比定性,外标法定量。结果表明,DIHP和DHNUP的线性范围均为0.40~4.0 mg·L^(-1),检出限(3S/N)为1.0~2.0 mg·kg^(-1)。按标准加入法进行回收试验,回收率在88.6%~115%之间,相对标准偏差(n=6)均小于5.0%。A method for the determination of DIHP and DHNUP in plastic products by gas chromatographymass spectrometry（GC-MS）was proposed.DIHP and DHNUP in the sample（0.500 0 g）were extracted by microwave extraction at 100℃for 30 min using 20 mL of ethyl acetate as extraction solvent,and then 2.0 mL of the extract was taken,made its volume up to 5.0 mL with ethyl acetate and filtrated.DIHP and DHNUP were analyzed by GC-MS under selected ion monitor（SIM）mode.The abundance ratio of the characteristic fragment ions was adopted for qualitative analysis,and the external standard method was adopted for quantification.As shown by the results,linear ranges of DIHP and DHNUP were both 0.40-4.0 mg·L^-1,with detection limits（3 S/N）ranged from 1.0 mg·kg^-1 to 2.0 mg·kg^-1.Test for recovery was made by standard addition method,giving results in the range of 88.6%^-115%,with RSDs（n=6）all less than 5.0%.

关 键 词：气相色谱-质谱法 微波萃取 1 2-苯二酸-二烷基酯 DIHP DHNUP 塑料制品 

分 类 号：O657.63[理学—分析化学]